Water → N-benzhydryl-4-(bromomethyl)benzenesulfonamide

HRID 40790

反応式

HRID 40790 の反応式
[CH:1]([NH2:14])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[Br:22][CH2:23][C:24]1[CH:29]=[CH:28][C:27]([S:30](Cl)(=[O:32])=[O:31])=[CH:26][CH:25]=1.O>ClCCl>[CH:1]([NH:14][S:30]([C:27]1[CH:26]=[CH:25][C:24]([CH2:23][Br:22])=[CH:29][CH:28]=1)(=[O:31])=[O:32])([C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 7036BenzhydrylamineHCID 8471TriethylamineHCID 27344094-(Bromomethyl)benzenesulfonyl chloride

生成物 1

HCID 67021864N-benzhydryl-4-(bromomethyl)benzenesulfonamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Benzhydrylamine (640 μL) was dissolved in dichloromethane (5.0 mL). To the solution, triethylamine (645 μl) and 4-(bromomethyl)benzenesulfonyl chloride (1.0 g) were added at 0° C., and the mixture was stirred at room temperature for 2 hours. To the reaction mixture, water (10 mL) was added, and the resultant mixture was then extracted with chloroform (30 mL). The organic layer was washed with brine (15 mL), dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (40% ethyl acetate/hexane) to obtain the title compound (753 mg).

後処理

  1. extractionthe resultant mixture was then extracted with chloroform (30 mL)
  2. washThe organic layer was washed with brine (15 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (40% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-39757e3b8a604a86b768458e01915af5
出典データセット
uspto-grants-2013_09
特許番号
US08530490B2

関連ノート

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